CN110093467B - Preparation method of iron coke - Google Patents

Preparation method of iron coke Download PDF

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CN110093467B
CN110093467B CN201910486421.2A CN201910486421A CN110093467B CN 110093467 B CN110093467 B CN 110093467B CN 201910486421 A CN201910486421 A CN 201910486421A CN 110093467 B CN110093467 B CN 110093467B
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iron
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CN110093467A (en
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储满生
鲍继伟
柳政根
王宏涛
赵伟
唐珏
韩冬
曹来更
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/04—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of powdered coal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/08—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form in the form of briquettes, lumps and the like
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B5/00—Making pig-iron in the blast furnace

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Abstract

A process for preparing ferro coke from CO2Dry distilling the iron coke green ball in the mixed atmosphere of COPreparing iron coke by physical treatment, in the mixed atmosphere, CO2The partial pressure of the gas is below 10%; the iron coke green ball is a pressed block formed by mixing and pressing coal powder and iron ore powder. Simple process operation, and can effectively prevent the iron coke from generating cracks and being coated with CO in the carbonization process2The corrosion phenomenon improves the mechanical strength and the yield of the iron coke.

Description

Preparation method of iron coke
Technical Field
The invention belongs to the technical field of ferrous metallurgy, and particularly relates to a preparation method of iron coke.
Background
The iron coke is used as a novel composite iron-making furnace charge, and has the advantages of wide raw material source, high comprehensive resource utilization rate, reduction of blast furnace fuel ratio and reduction of CO2The advantages of emission and the like become the hot point of research of Chinese and foreign scholars. The ferro coke is a carbon-iron composite furnace charge prepared by uniformly mixing iron-containing substances with coal and then carrying out molding and dry distillation and carbonization treatment on the mixture by a coke oven or a shaft furnace. The raw materials for preparing the iron coke are iron-containing materials such as metallurgical iron-containing waste, low-grade iron ore, fine iron powder and the like, and non-coking coal powder such as weakly caking coal, non-caking coal and the like, so that the price is low, the raw material source is greatly improved, and the comprehensive utilization of the waste is greatly improved; and the ferro-coke has higher gasification reactivity and lower gasification reaction starting temperature, and can reduce the temperature of a hot reserve area, so that the ferro-coke replaces part of coke to participate in blast furnace smelting, the consumption of the coke can be reduced, the coke ratio is reduced, and CO is reduced2And (5) discharging.
At present, the preparation method of the iron coke mainly comprises two methods of hot press molding, coke oven or shaft furnace carbonization, cold press molding, coke oven or shaft furnace carbonization. The cold press molding process increases the mechanical strength of the ferro-coke by adding a binder, wherein the used binder mainly comprises an inorganic binder, an organic binder and a composite binder. However, it was found that during the carbonization of the ferro coke, the ferro coke is producedThe yield of the iron coke is reduced due to the fact that volatilization analysis is carried out, semicoke shrinkage and the iron ore reduction rate are too high, and the mechanical strength of the iron coke cannot meet the production requirement; and the carbonization atmosphere adopted in the carbonization treatment process of the ferro coke contains more CO2The presence of CO in the atmosphere of iron coke and charring2A gasification reaction occurs and thus the material is corroded.
Therefore, in view of the above problems, a reasonable method for carbonizing ferro coke is needed.
Disclosure of Invention
Technical problem to be solved
In order to solve the above problems of the prior art, the present invention provides a method for preparing ferro coke. Simple process operation, and can effectively prevent the iron coke from generating cracks and being coated with CO in the carbonization process2The corrosion phenomenon improves the mechanical strength and the yield of the iron coke.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a process for preparing ferro coke from CO2Carrying out dry distillation treatment on the ferro-coke green ball in a mixed atmosphere of CO to prepare ferro-coke, wherein in the mixed atmosphere, CO is used for preparing the ferro-coke2The partial pressure of the gas is below 10%; the iron coke green ball is a pressed block formed by mixing and pressing coal powder and iron ore powder.
As an improvement of the preparation method of the ferro-coke, the conditions of the dry distillation treatment are as follows: heating the iron coke green ball from room temperature to 530-600 ℃ at a heating rate of 3-5 ℃/min, heating from 530-600 ℃ to 900-1100 ℃ at a heating rate of 5-7 ℃/min, and keeping the temperature for 3-5 h.
As an improvement of the preparation method of the ferro-coke, the preparation method of the ferro-coke green ball comprises the following steps: mixing and heating iron ore powder, bituminous coal and anthracite to obtain a first mixture; according to the mass percentage, the iron ore powder accounts for 10% -40%, the bituminous coal accounts for 55% -80%, and the anthracite coal accounts for 5% -10% in the first mixture; spraying hot asphalt binder which accounts for 5-7% of the mass of the first mixture into the first mixture, and uniformly mixing to obtain a second mixture; and pressing and molding the second mixture to obtain the iron coke green ball.
As an improvement of the preparation method of the iron coke, the hot asphalt binder is prepared by adopting asphalt heated by steam, and the heating temperature is 60-150 ℃.
As an improvement of the preparation method of the ferro-coke, the granularity of iron ore powder is below 1mm, and the granularity of coal powder is below 4 mm.
As an improvement of the preparation method of the ferro-coke, the compression molding adopts double-roll compression, and the pressure of the compression molding is 3 t/cm-6 t/cm.
As an improvement of the preparation method of the iron coke, the compression strength of the iron coke green ball is not lower than 900N, and the falling strength of the iron coke green ball is not lower than 15 times per ball.
(III) advantageous effects
The invention has the beneficial effects that:
1. controlling CO in a destructive distillation atmosphere2The partial pressure of the gas is below 10 percent, so that the occurrence of carbon gasification melting loss reaction is reduced, and the metallurgical performance of the iron coke is improved.
2. Before 550 ℃, the temperature rise rate is selected to be 3-5 ℃/min, so that the generation of cracks and the reduction of strength caused by violent decomposition and depolymerization of coal are greatly weakened; when the semi-coke is heated from 550 ℃ to 1000 ℃, the temperature rise rate is selected to be 5-7 ℃/min, so that the semi-coke shrinkage and the excessive shrinkage stress caused by iron ore reduction are greatly weakened. Therefore, the mechanical strength and the yield of the iron coke are improved, and the subsequent application of the iron coke is guaranteed.
Detailed Description
For the purpose of better explaining the present invention, the present invention will be described in detail by way of specific embodiments for easy understanding.
The percentage amounts referred to in the embodiments of the present invention are, unless otherwise specified, percent amounts by weight.
The invention provides a preparation method of iron coke, which specifically comprises the following steps:
step S1, preparation of iron coke green balls: uniformly mixing iron ore powder and coal powder according to 10-40% of iron ore powder, 55-80% of bituminous coal and 5-10% of anthracite, and heating to 60-150 ℃ to obtain a first mixture; spraying steam-heated asphalt accounting for 5-7% of the mass of the first mixture into the first mixture, and uniformly mixing to obtain a second mixture; and carrying out double-roller pressing molding on the second mixture at the pressure of 3-6 t/cm to obtain the iron coke green ball.
The soft coal and the anthracite are non-coking coals and are used as raw materials for preparing the iron coke, so that the cost is low, and the raw material source and the comprehensive utilization of waste materials are greatly improved. The uniformly mixed iron ore powder and coal powder are heated, so that the asphalt is added into the first mixture and still has good fluidity, and uniform mixing of the asphalt and the first mixture is promoted.
Preferably, the granularity of the iron ore powder is below 1mm, and the granularity of the coal powder is below 4 mm. Further preferably, the compression strength of the iron coke green ball is not lower than 900N, and the falling strength of the iron coke green ball is not lower than 15 times per ball, so that the iron coke green ball is ensured not to deform and break in the transportation, loading and unloading processes before entering the shaft furnace.
Step S2, preparation of iron coke products: charging the ferro-coke green pellets into a shaft furnace in CO2Dry distillation is carried out in a mixed atmosphere with CO2The partial pressure of the gas is below 10%; and heating the iron coke green ball from room temperature to 530-600 ℃ in the shaft furnace at the heating rate of 3-5 ℃/min, then heating from 530-600 ℃ to 900-1100 ℃ at the heating rate of 5-7 ℃/min, then keeping the temperature for 3-5 h, and cooling to obtain the iron coke product.
Controlling CO in a destructive distillation atmosphere2The partial pressure of the gas is below 10 percent, so that the occurrence of carbon gasification melting loss reaction is reduced, and the metallurgical performance of the iron coke is improved. In addition, the applicant researches and discovers that in the dry distillation process of the iron coke green pellets, before the temperature is 550 ℃, coal is decomposed and depolymerized violently, a large amount of tar and gas are separated out, almost all tar is separated out at the stage, the temperature rise speed is too high, cracks can be generated, the strength of the cracks is damaged, and the applicant optimally selects an appropriate temperature rise speed range to be 3-5 ℃/min; the temperature is increased from 550 ℃ to 1000 ℃, semicoke shrinkage and iron ore reduction can be generated, the temperature is increased too fast, the shrinkage stress is larger, and the applicant optimally selects an appropriate temperature increase rate range to be 5-7 ℃/min.
In conclusion, the invention considers the influence of the carbonization heating system and the carbonization atmosphere on the metallurgical performance of the iron coke aiming at the decomposition thermal decomposition characteristic of the iron coke, and the carbonization atmosphere only needs to consider CO2And CO in the CO mixed gas2The effect of partial pressure. The invention has simple process operation and obvious effect, and can effectively prevent the iron coke from generating cracks and CO in the carbonization process2The corrosion phenomenon improves the mechanical strength and the yield of the iron coke and provides guarantee for the application of the subsequent iron coke.
In the embodiment of the invention, the chemical components of the used iron ore powder are shown in the table 1, and the iron ore powder with the granularity of less than 0.074mm accounts for 80 percent; the industrial analysis of the bituminous coal and anthracite used is shown in table 2, and the particle size of the coal powder of the bituminous coal and the anthracite is below 4 mm; the binder used is preferably asphalt, and cellulose and high molecular weight polymers are used as the binder, and similar effects can be achieved.
TABLE 1 iron ore powder chemical composition (weight%/%)
Figure BDA0002085545390000041
TABLE 2 Industrial analysis of coal dust (weight%/%)
Figure BDA0002085545390000042
Figure BDA0002085545390000051
The influence of a carbonization temperature-raising system on the metallurgical performance of the iron coke in the preparation process of the iron coke is as follows:
comparative example 1
The embodiment provides a preparation method of ferro coke, which comprises the following steps:
step S1, preparation of iron coke green balls: uniformly mixing iron ore powder and coal powder according to 30% of iron ore powder, 55% (bituminous coal 1+ bituminous coal 2), 5% of anthracite and 10% of bituminous coal 3, and heating to 60 ℃ to obtain a first mixture; spraying steam-heated asphalt accounting for 5% of the mass of the first mixture into the first mixture, and uniformly mixing to obtain a second mixture; and carrying out double-roller pressing forming on the second mixture at the pressure of 6t/cm to obtain the iron coke green ball.
Step S2, putting the iron coke green pellets into a shaft furnace, and performing dry distillation in a nitrogen atmosphere; heating the iron coke green ball from room temperature to 550 ℃ in a shaft furnace at the heating rate of 3 ℃/min, then heating from 550 ℃ to 1000 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 4h, and cooling to obtain an iron coke product.
The test shows that the compression strength of the iron coke product in the comparative example 1 is 3977N, and the tumbling index of the type I
Figure BDA0002085545390000052
The content of the acid-resistant lubricating oil is 83.4%,
Figure BDA0002085545390000053
the tumbler index is 86.5 percent, the carbonization weight loss rate is 29.5 percent, and the yield is 100 percent.
Comparative example 2
The embodiment provides a preparation method of ferro coke, which comprises the following steps:
step S1, iron coke green pellets were prepared in the same manner as in comparative example 1.
Step S2, putting the iron coke green pellets into a shaft furnace, and performing dry distillation in a nitrogen atmosphere; heating the iron coke green ball from room temperature to 550 ℃ in a shaft furnace at the heating rate of 7 ℃/min, then heating from 550 ℃ to 1000 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 4h, and cooling to obtain an iron coke product.
The test shows that the compression strength of the iron coke product in the comparative example 2 is 3759N, and the tumbling index of the type I
Figure BDA0002085545390000054
The content of the organic acid is 82.4%,
Figure BDA0002085545390000055
the drum index is 84.6%, the carbonization weight loss rate is 30.1%, and the yield is 74%.
Comparative example 3
The embodiment provides a preparation method of ferro coke, which comprises the following steps:
step S1, iron coke green pellets were prepared in the same manner as in comparative example 1.
Step S2, putting the iron coke green pellets into a shaft furnace, and performing dry distillation in a nitrogen atmosphere; heating the iron coke green ball from room temperature to 550 ℃ in a shaft furnace at the heating rate of 7 ℃/min, then heating from 550 ℃ to 1000 ℃ at the heating rate of 9 ℃/min, then keeping the temperature for 4h, and cooling to obtain an iron coke product.
The test shows that the compression strength of the iron coke product in the comparative example 3 is 3545N, and the tumbling index of the type I
Figure BDA0002085545390000061
The content of the active carbon is 76.2%,
Figure BDA0002085545390000062
the drum index is 79.4 percent, the carbonization weight loss rate is 29.3 percent, and the yield is 62 percent.
Comparing comparative example 1 with comparative example 2 and comparative example 3, it can be seen that heating from room temperature to 550 ℃ at a heating rate of 3-5 ℃/min, and then heating from 550 ℃ to 1000 ℃ at a heating rate of 5-7 ℃/min can effectively prevent cracks from being generated in the iron coke carbonization process, and improve the mechanical strength and yield of the iron coke.
The influence of the carbonization atmosphere on the metallurgical performance of the iron coke in the preparation process of the iron coke is as follows:
example 1
The embodiment provides a preparation method of ferro coke, which comprises the following steps:
step S1, iron coke green pellets were prepared in the same manner as in comparative example 1.
Step S2, preparation of iron coke products: charging the ferro-coke green pellets into a shaft furnace in CO2Dry distillation with CO in a mixed atmosphere2The partial pressure of the gas was 10%; heating the iron coke green ball from room temperature to 550 ℃ in a shaft furnace at the heating rate of 3 ℃/min, then heating from 550 ℃ to 1000 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 4h, and cooling to obtain an iron coke product.
The iron coke product of example 1 was tested for compression resistanceStrength 3542N, type I tumbler index
Figure BDA0002085545390000063
The content of the active carbon is 80.3 percent,
Figure BDA0002085545390000064
the tumbler index is 83.5 percent, the carbonization weight loss rate is 31.5 percent, and the yield is 100 percent.
Example 2
The embodiment provides a preparation method of ferro coke, which comprises the following steps:
step S1, iron coke green pellets were prepared in the same manner as in comparative example 1.
Step S2, preparation of iron coke products: charging the ferro-coke green pellets into a shaft furnace in CO2Dry distillation with CO in a mixed atmosphere2The partial pressure of the gas was 7.5%; heating the iron coke green ball from room temperature to 550 ℃ in a shaft furnace at the heating rate of 3 ℃/min, then heating from 550 ℃ to 1000 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 4h, and cooling to obtain an iron coke product.
The test shows that the compression strength of the iron coke product in example 2 is 3603N, and the drum index of type I
Figure BDA0002085545390000071
The content of the organic acid was 81.1%,
Figure BDA0002085545390000072
the tumbler index is 83.9 percent, the carbonization weight loss rate is 31.0 percent, and the yield is 100 percent.
Example 3
The embodiment provides a preparation method of ferro coke, which comprises the following steps:
step S1, iron coke green pellets were prepared in the same manner as in comparative example 1.
Step S2, preparation of iron coke products: charging the ferro-coke green pellets into a shaft furnace in CO2Dry distillation with CO in a mixed atmosphere2The partial pressure of the gas was 5%; the iron coke green ball is heated from room temperature to 550 ℃ in a shaft furnace at the heating rate of 3 ℃/min, and then is heated from 550 ℃ at the heating rate of 5 ℃/minKeeping the temperature for 4 hours after the temperature reaches 1000 ℃, and obtaining the ferro-coke product after cooling.
The test shows that the compression strength of the iron coke product in example 3 is 3692N, and the drum index of type I
Figure BDA0002085545390000073
The content of the organic acid is 82.1%,
Figure BDA0002085545390000074
the drum index is 84.6%, the carbonization weight loss rate is 30.3%, and the yield is 100%.
Examples 1, 2, 3 were compared with comparative example 1. It is understood that the weight loss rates of the iron coke in examples 1 to 3 are 31.5%, 31.0% and 30.3%, respectively, which is comparable to the weight loss rate of the iron coke in the nitrogen atmosphere (in which no carbon gasification reaction occurs) of 30.1%; shows that the control of CO in the dry distillation atmosphere2The partial pressure of the gas is below 10 percent, so that the occurrence of carbon gasification reaction is reduced, the weight loss rate of the iron coke is reduced, and the weight loss rate of the iron coke is almost equivalent to the weight loss rate of the iron coke during dry distillation under the protection of nitrogen atmosphere.
Comparative example 4
The comparative example provides a method for preparing ferro-coke, which comprises the following steps:
step S1, iron coke green pellets were prepared in the same manner as in comparative example 1.
Step S2, preparation of iron coke products: charging the ferro-coke green pellets into a shaft furnace in CO2Dry distillation with CO in a mixed atmosphere2The partial pressure of the gas was 15%; heating the iron coke green ball from room temperature to 550 ℃ in a shaft furnace at the heating rate of 3 ℃/min, then heating from 550 ℃ to 1000 ℃ at the heating rate of 5 ℃/min, keeping the temperature for 4h, and cooling to obtain an iron coke product.
The test shows that the compression strength of the ferro coke product in the comparative example 4 is 2918N, and the tumbling index of the type I
Figure BDA0002085545390000075
The content of the active carbon is 75.2%,
Figure BDA0002085545390000076
the tumbler index is 80.3 percent, the carbonization weight loss rate is 36.7 percent, and the yield is 83 percent.
As compared with example 1, it can be seen that CO is present in the dry distillation atmosphere2When the partial pressure of the gas is more than 10 percent, the carbonization weight loss rate is higher, which indicates that CO is generated in the dry distillation process of the ferro-coke2The corrosion condition is serious, so that the compressive strength and the yield of the iron coke are greatly reduced.
In conclusion, the compression strength of the iron coke prepared by the method is not lower than 3100N, and the type I barrate index
Figure BDA0002085545390000081
Not less than 80 percent,
Figure BDA0002085545390000082
the drum index is not less than 80%, the carbonization weight loss rate is below 31.5%, and the yield is 100%. Effectively prevent the iron coke from generating cracks and being coated with CO in the carbonization process2Corrosion, and the mechanical strength and yield of the ferro coke are improved.
It should be understood that the above description of specific embodiments of the present invention is only for the purpose of illustrating the technical lines and features of the present invention, and is intended to enable those skilled in the art to understand the contents of the present invention and to implement the present invention, but the present invention is not limited to the above specific embodiments. It is intended that all such changes and modifications as fall within the scope of the appended claims be embraced therein.

Claims (7)

1. The preparation method of the ferro coke is characterized in that the ferro coke is prepared from CO2Carrying out dry distillation treatment on the ferro-coke green ball in a mixed atmosphere of CO to prepare ferro-coke, wherein in the mixed atmosphere, CO is used for preparing the ferro-coke2The partial pressure of the gas is below 10%; the iron coke green ball is a pressed block formed by mixing and pressing coal powder and iron ore powder;
the dry distillation treatment conditions are as follows:
heating the iron coke green ball from room temperature to 530-600 ℃ at a heating rate of 3-5 ℃/min, then heating from 530-600 ℃ to 900-1100 ℃ at a heating rate of 5-7 ℃/min, and then keeping the temperature for 3-5 h;
the preparation method of the iron coke green ball comprises the following steps:
mixing and heating iron ore powder, bituminous coal and anthracite to obtain a first mixture; according to the mass percentage, the iron ore powder accounts for 10% -40%, the bituminous coal accounts for 55% -80%, and the anthracite coal accounts for 5% -10% in the first mixture;
uniformly mixing the first mixture with a binder to obtain a second mixture, wherein the binder is an asphalt binder or a high molecular polymer binder;
and pressing and molding the second mixture to obtain the iron coke green ball.
2. The method according to claim 1, wherein the binder based on a high molecular polymer is a cellulose-based binder.
3. The method according to claim 1, wherein the hot asphalt binder is sprayed into the first mixture in an amount of 5 to 7% by mass of the first mixture and uniformly mixed to obtain a second mixture.
4. The method for preparing ferro-coke according to claim 3, wherein the hot asphalt binder is prepared by heating asphalt with steam at a temperature of 60 to 150 ℃.
5. The method according to claim 1, wherein the iron ore powder has a particle size of 1mm or less, and the pulverized coal has a particle size of 4mm or less.
6. The method for preparing ferro-coke according to claim 1, wherein the pressing is performed by a double-roll pressing process, and the pressure of the double-roll pressing is 3t/cm to 6 t/cm.
7. The method for producing ferro-coke according to claim 1, wherein the compressive strength of the ferro-coke green pellets is not less than 900N, and the falling strength of the ferro-coke green pellets is not less than 15 times per pellet.
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